CN106841186A - A kind of method of quick detection pymetrozine - Google Patents
A kind of method of quick detection pymetrozine Download PDFInfo
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- CN106841186A CN106841186A CN201710075857.3A CN201710075857A CN106841186A CN 106841186 A CN106841186 A CN 106841186A CN 201710075857 A CN201710075857 A CN 201710075857A CN 106841186 A CN106841186 A CN 106841186A
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- pymetrozine
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- mixed liquor
- aqueous solution
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- 239000005925 Pymetrozine Substances 0.000 title claims abstract description 127
- QHMTXANCGGJZRX-WUXMJOGZSA-N pymetrozine Chemical compound C1C(C)=NNC(=O)N1\N=C\C1=CC=CN=C1 QHMTXANCGGJZRX-WUXMJOGZSA-N 0.000 title claims abstract description 127
- 238000001514 detection method Methods 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 58
- 230000008859 change Effects 0.000 claims abstract description 50
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 49
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000010931 gold Substances 0.000 claims abstract description 41
- 229910052737 gold Inorganic materials 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 38
- 239000002105 nanoparticle Substances 0.000 claims abstract description 33
- 238000010521 absorption reaction Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 156
- 239000007864 aqueous solution Substances 0.000 claims description 63
- 230000004048 modification Effects 0.000 claims description 49
- 238000012986 modification Methods 0.000 claims description 49
- 239000001509 sodium citrate Substances 0.000 claims description 31
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 24
- 230000000052 comparative effect Effects 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 244000269722 Thea sinensis Species 0.000 claims description 14
- 235000009569 green tea Nutrition 0.000 claims description 14
- 235000019987 cider Nutrition 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000007306 functionalization reaction Methods 0.000 claims description 10
- 239000001508 potassium citrate Substances 0.000 claims description 7
- 229960002635 potassium citrate Drugs 0.000 claims description 7
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 7
- 235000011082 potassium citrates Nutrition 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000012488 sample solution Substances 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 2
- 238000005829 trimerization reaction Methods 0.000 claims 2
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims 1
- 241001124076 Aphididae Species 0.000 claims 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 239000011260 aqueous acid Substances 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 125000000168 pyrrolyl group Chemical group 0.000 claims 1
- 230000009471 action Effects 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 230000009467 reduction Effects 0.000 description 38
- 235000011083 sodium citrates Nutrition 0.000 description 30
- 238000002360 preparation method Methods 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 150000007974 melamines Chemical class 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 8
- 235000013339 cereals Nutrition 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000012279 sodium borohydride Substances 0.000 description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 239000002917 insecticide Substances 0.000 description 5
- 235000015165 citric acid Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910003803 Gold(III) chloride Inorganic materials 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 235000021393 food security Nutrition 0.000 description 2
- 235000015203 fruit juice Nutrition 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- QMNWYGTWTXOQTP-UHFFFAOYSA-N 1h-triazin-6-one Chemical compound O=C1C=CN=NN1 QMNWYGTWTXOQTP-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 241000251539 Vertebrata <Metazoa> Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001736 differential pulse polarography Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical class [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of detection method of pymetrozine in water solution system, there is specific hydrogen bond action in the golden nanometer particle that the method is based on pymetrozine and can be modified with melamine, the resonance of golden nanometer particle surface plasma is caused to change, the color of solution of gold nanoparticles and ultravioletvisible absorption intensity, peak value is set to change, therefore the color change of solution is directly observed by the naked eye, whether pymetrozine can be contained in quick detection solution, it is high with simple to operate, low cost, sensitivity, the advantages of applied widely.The nano material can realize to pymetrozine it is real-time, quickly detect.
Description
Technical field
The present invention relates to the detection technique of pymetrozine, more particularly to a kind of water that is quick, easily identifying complicated component
The detection method of the pymetrozine of low concentration in solution.
Background technology
Cereal crops, vegetables and fruit Isoquant and quality are improved to reduce pest and disease damage, chemical insecticide extensively should
With.However, the insecticide of residual can be polluted to soil, water environment and food etc., threat is brought to the survival and development of the mankind.
Therefore, accurate detection insecticide residues causes the extensive attention of people.
Pymetrozine belongs to pyridines or Triazinone insecticide, is brand-new non-killing livestock property insecticide, earliest by Switzerland one
Company developed in 1988, and the product shows excellent prevention effect to the sucking pest of various crop, and right
People, birds and vertebrate toxicity are relatively low.Even so, Environmental protection mechanism is still classified as pymetrozine potentially
Carcinogen.Excess free enthalpy pymetrozine can cause the symptoms such as headache, Nausea and vomiting, particularly to patients such as hypertension, heart diseases
Harm is bigger.The maximum intake of China's food security standard pymetrozine is 138nM (0.03mg/kg).Therefore, simple and quick inspection
The residual for surveying pymetrozine is extremely important.
At present detection pymetrozine method mainly have high performance liquid chromatography (HPLC, Environmental Pollution and Control, 2008,30,
40-42；Pesticide Science journal, 2011,13,547-550), liquid phase-mass spectrum be used in conjunction method (J.Agric.Food Chem.2008,56,
6851-6856.), gas chromatography (Food Chem.2014,146,448-454), electrochemical process (Anal.Methods,
2015,7,9100-9107), differential pulse polarography (J.Hazard.Mater.2007,141,700-706) etc., though these methods
It is so safe and reliable, but detection process is complicated, expends the time long.Up to the present, only two documents have been reported for work and have utilized gold nano
Particle colorimetric detection pymetrozine, but its detection limit for height, sensitive difference, selectively bad (Appl.Mech.Mater.2011,117,
958-961；Micro Nano Lett.2010,5,304-308).Because these detection liquid building-up processes are complicated, poor repeatability,
Cause that the pymetrozine for realizing the aqueous solution is quick, timely Site Detection method is difficult to.
The present invention modifies gold nano grain for the deficiency of above-mentioned detection method using melamine, is lured based on pymetrozine
Lead the gold nano grain after modification to reunite, cause color change, so as to realize the quantitative determination to pymetrozine.Detection of the invention
Method has the features such as simple, quick, selectivity is high, sensitivity is good.
The content of the invention
The problem to be solved in the present invention is directed to above-mentioned technical problem, a kind of quick, accurate and easy inspection of invention
The method for measuring pymetrozine in the aqueous solution, the method is applicable not only to the detection of pymetrozine in the aqueous solution, and can be used to examine
The pymetrozine surveyed in fruit juice, green tea solution.
The present invention solves the technical scheme taken of above-mentioned technical problem：A kind of method for detecting pymetrozine, using three
The amine-modified golden nanometer particle of paracyanogen, prepares the golden nanometer particle of functionalization, can occur with melamine by pymetrozine specific
Hydrogen bond action so that solution colour changes, cause golden nanometer particle surface etc. so as to cause the reunion of golden nanometer particle
The peak position and absorption intensity of ion resonance absworption peak change (Fig. 1), realize quick, letter to pymetrozine in the aqueous solution
Just, accurately detection.
A kind of method of quick detection pymetrozine that the present invention is provided, comprises the following steps：
(1) certain density aqueous solution of chloraurate is added in round-bottomed flask, boiling is heated with stirring to, reduction is rapidly joined
Agent, after reaction certain hour, is obtained specific morphology and the golden nanometer particle aqueous solution with a certain size size；
(2) in the case of stirring, it is added dropwise in the golden nanometer particle aqueous solution obtained in step (1) certain density
Melamine solution, obtains final product the functionalization golden nanometer particle aqueous solution of melamine modification after reaction certain hour；
(3) the functionalization golden nanometer particle aqueous solution conduct of melamine modification obtained in two parts of isometric steps (2) is taken
Detection liquid；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and isometric with comparative solution is treated
Detection solution is separately added into the detection liquid described in two parts, forms the first mixed liquor and the second mixed liquor；
(4) color of the second mixed liquor of contrast and the first mixed liquor, if there is color change, exists in solution to be detected
Pymetrozine, if not existing color change, does not exist pymetrozine in solution to be detected, or, contrast the second mixed liquor and first
The ultravioletvisible absorption intensity of mixed liquor, peak value, if its ultravioletvisible absorption intensity, peak value change, solution to be detected
In there is pymetrozine, if not changing, in solution to be detected do not exist pymetrozine.
If preferably, the figure that can reflect pymetrozine concentration and solution colour variation relation in solution can be provided
Piece, then the solution colour change picture of the second mixed liquor that can be obtained by the present invention is compared with the picture of the standard,
So as to obtain the concentration of pymetrozine in the second mixed liquor.The picture preparation method of the standard is as follows：
The compound method for being first according to the second described mixed liquor prepares a series of aqueous solution of different pymetrozine concentration, point
The color change of golden nanometer particle that the pymetrozine of various concentrations causes Fan Ying be observed, in this, as colorimetric after a period of time
Standard card.
In such scheme, it is preferable that the concentration of aqueous solution of chloraurate described in step (1) is 1~5mM, the reaction time is
10~30min.
Preferably, the concentration of melamine solution described in step (2) is 1~5 μM, and the reaction time is 10~30min.
Preferably, the reducing agent be sodium borohydride, sodium citrate, potassium citrate in one or several.
Preferably, the pH scopes of the functionalization golden nanometer particle aqueous solution of the melamine modification are between 3~6.5.
Preferably, the solution to be detected is obtained for polymer solution in water, lake water solution or foodstuff samples after treatment
Sample solution.
It is further preferred that the sample solution that the foodstuff samples are obtained after treatment is green tea or cider (figure
2)。
In sum, the invention provides a kind of method for detecting pymetrozine in the aqueous solution, the method is based on reuniting
Mechanism, Au-N keys can be formed using melamine with golden nanometer particle, and pymetrozine can occur specifically with melamine
Hydrogen bond action so that solution colour changes golden nanometer particle because of reunion, causes golden nanometer particle surface plasma resonance
The peak position and absorption intensity of absworption peak change (Fig. 1), therefore, directly carried out using naked eyes and UV, visible light spectrophotometric
Judge, you can be quickly detected from whether containing pymetrozine in solution, realize in solution pymetrozine it is quick, easy, real-time
Detection.
Preferably, the material for participating in reaction is that chemistry is pure.
Compared with prior art, the advantage of the invention is that：The detection method of the pymetrozine that the present invention is provided is simple to operate
Conveniently, detect that quick, with low cost, sensitivity is high and can operate on the spot at the scene, it is adaptable to the quick inspection of food security
Survey, the detection of pymetrozine, is with a wide range of applications in monitoring domestic water and the various water samples for obtaining after treatment.
Brief description of the drawings
Fig. 1 is the uv absorption spectra of the functionalization golden nanometer particle aqueous solution of the invention；Wherein (a) is melamine
Golden nanometer particle aqueous solution ultra-violet absorption spectrum after modification；B () is the gold nano after the melamine modification containing pymetrozine
Particle aqueous solution ultra-violet absorption spectrum；
Fig. 2 be running water, lake water, green tea and in cider solution pymetrozine detection picture；Wherein PYM is pymetrozine
Abbreviation.
Specific embodiment
The present invention is further described below by specific embodiment, but does not limit present disclosure.
Embodiment 1
(1) preparation of the golden nanometer particle of the reduction of sodium citrate of melamine modification
The preparation of (a) gold nano grain, 10mL 5mM AuCl3·HCl·4H2O adds 85mL ultrapure under agitation
In water, it is heated to boiling, rapidly joins the sodium citrate solution that 5mL mass fractions are 1%, continues heating stirring to solution colour
Become colorless by light yellow, after eventually becoming claret, stop heating stirring, standing is cooled to room temperature, is put into 4 DEG C of refrigerator
Preserve；
B () takes the golden nanometer particle aqueous solution prepared in 20mL steps (a), under agitation, be dropwise added dropwise the three of 4 μM
Paracyanogen amine aqueous solution, continues to stir 10min, you can obtain the solution of gold nanoparticles of the reduction of sodium citrate of melamine modification, and
As detection solution；
(2) in solution pymetrozine detection
A () takes the reduction of sodium citrate that two parts of isometric melamines are modified in the obtained detection liquid of step (1)
Solution of gold nanoparticles；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and with comparative solution etc.
The solution to be detected of volume is separately added into the solution of gold nanoparticles of the reduction of sodium citrate of described two parts of melamines modification
In, form the first mixed liquor and the second mixed liquor；
B after () reaction 10min, the color of the second mixed liquor of contrast and the first mixed liquor is to be checked if there is color change
Survey in solution and there is pymetrozine, if not existing color change, do not exist pymetrozine in solution to be detected, or, contrast second
Ultravioletvisible absorption intensity, the peak value of mixed liquor and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value change,
Then there is pymetrozine in solution to be detected, if not changing, do not exist pymetrozine in solution to be detected.
Embodiment 2
(1) preparation of the golden nanometer particle of the sodium borohydride reduction of melamine modification
A the preparation of () gold nano grain, 4mL 1mM gold chlorides is added in 94mL ultra-pure waters, be heated to boiling, quickly
The sodium borohydride of 2mL 0.1M newly configurations is added, after question response 20min, the solution of gold nanoparticles of claret just can be obtained；
B () takes the solution of gold nanoparticles prepared in 70mL steps (a), under agitation, the μ of 20mL 4.0 are dropwise added dropwise
The melamine solution of M, continues to stir 30min, you can the golden nanometer particle for obtaining the sodium borohydride reduction of melamine modification is molten
Liquid, and as detection solution；
(2) in solution pymetrozine detection
A () takes the sodium borohydride reduction that two parts of isometric melamines are modified in the obtained detection liquid of step (1)
Solution of gold nanoparticles；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and with comparative solution etc.
The solution to be detected of volume is separately added into the solution of gold nanoparticles of the sodium borohydride reduction of described two parts of melamines modification
In, form the first mixed liquor and the second mixed liquor；
B after () reaction 25min, the color of the second mixed liquor of contrast and the first mixed liquor is to be checked if there is color change
Survey in solution and there is pymetrozine, if not existing color change, do not exist pymetrozine in solution to be detected, or, contrast second
Ultravioletvisible absorption intensity, the peak value of mixed liquor and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value change,
Then there is pymetrozine in the aqueous solution to be detected, if not changing, do not exist pymetrozine in the aqueous solution to be detected.
Embodiment 3
(1) preparation of the golden nanometer particle of the potassium citrate reduction of melamine modification
The preparation of (a) gold nano grain, by 10mL 3mM AuCl3·HCl·4H2O adds 85mL to surpass under agitation
In pure water, it is heated to boiling, rapidly joins the potassium citrate solution that 5mL mass fractions are 1%, continues heating stirring to solution face
Color is become colorless by light yellow, after eventually becoming claret, stops heating stirring, and standing is cooled to room temperature, is put into 4 DEG C of refrigerator
Middle preservation；
B () takes the solution of gold nanoparticles prepared in 70mL steps (a), under agitation, the μ of 20mL 4.0 are dropwise added dropwise
The melamine solution of M, continues to stir 20min, you can the golden nanometer particle for obtaining the potassium citrate reduction of melamine modification is molten
Liquid, and as detection solution；
(2) in solution pymetrozine detection
What a potassium citrate that () takes two parts of isometric melamine modifications in the obtained detection liquid of step (1) was reduced
Solution of gold nanoparticles；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and with comparative solution etc.
The solution to be detected of volume is separately added into the solution of gold nanoparticles of the potassium citrate reduction of described two parts of melamines modification
In, form the first mixed liquor and the second mixed liquor；
B after () reaction 20min, the color of the second mixed liquor of contrast and the first mixed liquor is to be checked if there is color change
Survey in solution and there is pymetrozine, if not existing color change, do not exist pymetrozine in solution to be detected, or, contrast second
Ultravioletvisible absorption intensity, the peak value of mixed liquor and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value change,
Then there is pymetrozine in solution to be detected, if not changing, do not exist pymetrozine in solution to be detected.
Embodiment 4
(1) pH is the preparation of the golden nanometer particle of the reduction of sodium citrate of 3 melamine modification
In Example 1 in step (1) melamine modification reduction of sodium citrate solution of gold nanoparticles 20mL, plus
It is 3 to enter appropriate hydrochloric acid solution regulation pH, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate of the melamine modification that two parts of isometric pH are 3 is measured in the obtained detection liquid of step (1)
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate of the melamine modification that two parts of described pH are 3
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reaction 30min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in the aqueous solution, if not existing color change, do not exist pymetrozine in the aqueous solution to be detected, or, contrast the
Ultravioletvisible absorption intensity, the peak value of two mixed liquors and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value become
Change, then there is pymetrozine in the aqueous solution to be detected, if not changing, do not exist pymetrozine in the aqueous solution to be detected.
Embodiment 5
(1) pH is the preparation of the golden nanometer particle of the reduction of sodium citrate of 4 melamine modification
In Example 1 in step (1) melamine modification reduction of sodium citrate solution of gold nanoparticles 20mL, plus
It is 4 to enter appropriate hydrochloric acid solution regulation pH, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate of the melamine modification that two parts of isometric pH are 4 is measured in the obtained detection liquid of step (1)
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate of the melamine modification that two parts of described pH are 4
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reaction 15min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in the aqueous solution, if not existing color change, do not exist pymetrozine in the aqueous solution to be detected, or, contrast the
Ultravioletvisible absorption intensity, the peak value of two mixed liquors and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value become
Change, then there is pymetrozine in the aqueous solution to be detected, if not changing, do not exist pymetrozine in the aqueous solution to be detected.
Embodiment 6
(1) pH is the preparation of the golden nanometer particle of the reduction of sodium citrate of 5 melamine modification
In Example 1 in step (1) melamine modification reduction of sodium citrate solution of gold nanoparticles 20mL, plus
It is 5 to enter appropriate hydrochloric acid solution regulation pH, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate of the melamine modification that two parts of isometric pH are 5 is measured in the obtained detection liquid of step (1)
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate of the melamine modification that two parts of described pH are 5
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reaction 15min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in the aqueous solution, if not existing color change, do not exist pymetrozine in the aqueous solution to be detected, or, contrast the
Ultravioletvisible absorption intensity, the peak value of two mixed liquors and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value become
Change, then there is pymetrozine in the aqueous solution to be detected, if not changing, do not exist pymetrozine in the aqueous solution to be detected.
Embodiment 7
(1) pH is the preparation of the golden nanometer particle of the reduction of sodium citrate of 6 melamine modification
In Example 1 in step (1) melamine modification reduction of sodium citrate solution of gold nanoparticles 20mL, plus
It is 6 to enter appropriate hydrochloric acid solution regulation pH, and as detection solution；
(2) in solution pymetrozine detection
The sodium citrate of the melamine modification that two parts of isometric pH are 6 is measured in the obtained detection liquid of step (1)
The solution of gold nanoparticles of reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric aqueous solution to be detected of solution is separately added into the reduction of sodium citrate of the melamine modification that two parts of described pH are 6
In solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reaction 15min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in the aqueous solution, if not existing color change, do not exist pymetrozine in the aqueous solution to be detected, or, contrast the
Ultravioletvisible absorption intensity, the peak value of two mixed liquors and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value become
Change, then there is pymetrozine in the aqueous solution to be detected, if not changing, do not exist pymetrozine in the aqueous solution to be detected.
Embodiment 8
(1) pH is the preparation of the golden nanometer particle of the reduction of sodium citrate of 6.5 melamine modification
In Example 1 in step (1) melamine modification reduction of sodium citrate solution of gold nanoparticles 20mL, plus
It is 6.5 to enter appropriate hydrochloric acid solution regulation pH, and as detection solution；
(2) in solution pymetrozine detection
The citric acid of the melamine modification that two parts of isometric pH are 6.5 is measured in the obtained detection liquid of step (1)
The solution of gold nanoparticles of sodium reduction；Prepare the aqueous solution solution as a comparison without pymetrozine, by comparative solution and with it is right
The to be detected aqueous solution more isometric than solution is separately added into the sodium citrate of the melamine modification that two parts of described pH are 6.5 also
In former solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reaction 15min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in the aqueous solution, if not existing color change, do not exist pymetrozine in the aqueous solution to be detected, or, contrast the
Ultravioletvisible absorption intensity, the peak value of two mixed liquors and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value become
Change, then there is pymetrozine in the aqueous solution to be detected, if not changing, do not exist pymetrozine in the aqueous solution to be detected.
Embodiment 9
The detection of pymetrozine in polymer solution in water
Two parts of citric acids of isometric melamine modification are measured in Example 1 in the obtained detection liquid of step (1)
The solution of gold nanoparticles of sodium reduction；Prepare the polymer solution in water solution as a comparison without pymetrozine, by comparative solution and
The to be detected polymer solution in water isometric with comparative solution is separately added into the sodium citrate of described two parts of melamines modification also
In former solution of gold nanoparticles, the first mixed liquor and the second mixed liquor are formed；
After reaction 25min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in polymer solution in water, if not existing color change, do not exist pymetrozine in polymer solution in water to be detected, or
Ultravioletvisible absorption intensity, the peak value of person, the second mixed liquor of contrast and the first mixed liquor, if its ultravioletvisible absorption intensity, peak
Value changes, then there is pymetrozine in polymer solution in water to be detected, if not changing, in polymer solution in water to be detected
In the absence of pymetrozine.
Embodiment 10
The detection of pymetrozine in lake water
Two parts of citric acids of isometric melamine modification are measured in Example 1 in the obtained detection liquid of step (1)
The solution of gold nanoparticles of sodium reduction；Prepare the lake water solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric lake water to be detected of solution is separately added into Jenner's grain of rice of the reduction of sodium citrate of described two parts of melamines modification
In sub- solution, the first mixed liquor and the second mixed liquor are formed；
After reaction 20min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in lake water, if not existing color change, do not exist pymetrozine in lake water to be detected, or, contrast second is mixed
Ultravioletvisible absorption intensity, the peak value of liquid and the first mixed liquor are closed, if its ultravioletvisible absorption intensity, peak value change,
There is pymetrozine in lake water to be detected, if not changing, do not exist pymetrozine in lake water to be detected.
Embodiment 11
(1) preparation of green tea solution
A little green tea is taken, 100 DEG C of water is added, 10min is stood, taken in the upper strata aqueous solution a to beaker, be cooled to room temperature,
Filtered using 0.22 μM of filter membrane, obtained green tea solution standby.
(2) in green tea pymetrozine detection
Two parts of citric acids of isometric melamine modification are measured in Example 1 in the obtained detection liquid of step (1)
The solution of gold nanoparticles of sodium reduction；Prepare the green tea solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric green tea solution to be detected of solution is separately added into the Jenner of the reduction of sodium citrate of described two parts of melamines modification
In rice corpuscles solution, the first mixed liquor and the second mixed liquor are formed；
After reaction 20min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in green tea, if not existing color change, do not exist pymetrozine in green tea to be detected, or, contrast second is mixed
Ultravioletvisible absorption intensity, the peak value of liquid and the first mixed liquor are closed, if its ultravioletvisible absorption intensity, peak value change,
There is pymetrozine in green tea to be detected, if not changing, do not exist pymetrozine in green tea to be detected.
Embodiment 11
(1) preparation of cider solution
Apple is enucleated, is squeezed the juice with juice extractor, fruit juice is put into centrifuge tube (8000rpm) 30min is centrifuged, taken
Clear liquid, is filtered using 0.22 μM of filter membrane, obtains cider standby.
(2) in cider pymetrozine detection
Two parts of sodium citrates of isometric melamine modification are taken in Example 1 in the obtained detection liquid of step (1)
The solution of gold nanoparticles of reduction；Prepare the cider solution as a comparison without pymetrozine, by comparative solution and with contrast
The isometric cider to be detected of solution is separately added into the gold nano of the reduction of sodium citrate of described two parts of melamines modification
In particle solution, the first mixed liquor and the second mixed liquor are formed；
After reaction 20min, the color of the second mixed liquor of contrast and the first mixed liquor is to be detected if there is color change
There is pymetrozine in cider, if not existing color change, do not exist pymetrozine in cider to be detected, or, contrast the
Ultravioletvisible absorption intensity, the peak value of two mixed liquors and the first mixed liquor, if its ultravioletvisible absorption intensity, peak value become
Change, then there is pymetrozine in cider to be detected, if not changing, do not exist pymetrozine in cider to be detected.
Embodiment described above has been described in detail to technical scheme, it should be understood that the above is only
It is specific embodiment of the invention, is not intended to limit the invention, all any modifications made in spirit of the invention
With improve etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of method of quick detection pymetrozine, it is characterised in that by the use of golden nanometer particle as main body, in Gold nanoparticle
Surface modification melamine, prepares the golden nanometer particle of functionalization；
It is as follows based on the functionalization golden nanometer particle specific detecting step of quick detection pymetrozine：
(1) certain density aqueous solution of chloraurate is added in round-bottomed flask, boiling is heated with stirring to, reducing agent is rapidly joined,
After reaction certain hour, the golden nanometer particle aqueous solution is obtained；
(2) in the case of stirring, certain density trimerization is added dropwise in the golden nanometer particle aqueous solution obtained in step (1)
Cyanamide solution, is obtained the functionalization golden nanometer particle aqueous solution of melamine modification after reaction certain hour；
(3) the functionalization golden nanometer particle aqueous solution of melamine modification obtained in two parts of isometric steps (2) is taken as detection
Liquid；The aqueous solution solution as a comparison without pymetrozine is prepared, by comparative solution and isometric with comparative solution to be detected
Solution is separately added into two parts of described detection liquid, forms the first mixed liquor and the second mixed liquor；
(4), if there is color change, there is pyrrole aphid in the color of the second mixed liquor of contrast and the first mixed liquor in solution to be detected
Ketone, if not existing color change, does not exist pymetrozine in solution to be detected, or, the second mixed liquor of contrast mixes with first
The ultravioletvisible absorption intensity of liquid, peak value, if its ultravioletvisible absorption intensity, peak value change, deposit in solution to be detected
In pymetrozine, if not changing, do not exist pymetrozine in solution to be detected.
2. a kind of method of quick detection pymetrozine as claimed in claim 1, it is characterised in that the gold of chlorine described in step (1)
The concentration of aqueous acid is 1~5mM, and the reaction time is 10~30min.
3. a kind of method of quick detection pymetrozine as claimed in claim 1, it is characterised in that trimerization described in step (2)
The concentration of cyanamide solution is 1~5 μM, and the reaction time is 10~30min.
4. a kind of method of quick detection pymetrozine as claimed in claim 1, it is characterised in that described reducing agent is boron hydrogen
Change sodium, sodium citrate, one or several in potassium citrate.
5. a kind of method of quick detection pymetrozine as claimed in claim 1, it is characterised in that the melamine modification
The pH scopes of the functionalization golden nanometer particle aqueous solution are between 3~6.5.
6. a kind of method of quick detection pymetrozine as claimed in claim 1, it is characterised in that the solution to be detected be from
Carry out the aqueous solution, the sample solution that lake water solution or foodstuff samples are obtained after treatment.
7. a kind of method of quick detection pymetrozine as claimed in claim 6, it is characterised in that the foodstuff samples are at
The sample solution obtained after reason is green tea solution or cider.
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